• Title/Summary/Keyword: LC/MS analysis

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Evaluation of Antioxidant, Cytoprotective and Antimicrobial Properties of Polygoni multiflori Radix Extract, Fractions and Its Major Constituent (하수오 추출물, 분획물 및 주성분의 항산화, 세포 보호 및 항균 활성에 관한 평가)

  • Shin, Hyuk Soo;Kim, Minwoo;Song, Jerry;Lee, Junseok;Ha, Yoonjeong;Jeon, Young Hee;Kim, Ji Woong;Lee, Yun Ju;Park, Soo Nam
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.44 no.4
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    • pp.407-417
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    • 2018
  • In this study, the antioxidant, cytoprotective and antimicrobial activities of 50% ethanol extract of Polygoni multiflori Radix (PMR) and its ethyl acetate fraction were evaluated to confirm the applicability as a functional ingredient. The activities of the major constituent of PMR were verified and 2, 3, 5, 4′-tetrahydroxystilbene 2-O-${\beta}$-D-glucoside (THSG) was confirmed to be the main component of extract and fraction using HPLC-DAD, LC-EIS-MS analysis. The phenolic and THSG contents of the ethyl acetate fraction were 11.1- and 3.0-folds higher than those of the ethanol extract, respectively. As a result of the DPPH assay and that of luminol dependent chemiluminescence assay in $Fe^{3+}$-EDTA/H2O2 system. the ethylacetate fraction was superior to the ethanol extract in free radical and ROS scavenging activities. Especially, the ethyl acetate fraction and THSG exhibited the similar scavenging activity like L-ascorbic acid in ROS scavenging activity. The ethyl acetate fraction perceived the most potent cytoprotective effect against oxidative damage of erythrocytes induced by photosensitization reaction, followed by the ethanol fraction, THSG and that of (+)-${\alpha}$-tocopherol, which was used as a positive control. Antimicrobial activities were evaluated by disc diffusion and broth microdilution assay against S. aureus, E. coli, P. aeruginosa and C. albicans. In particular, the antibacterial activity of the extract and fraction against S. aureus was superior to that of methyl paraben. Taken together, our results suggest that PMR could be used as a natural ingredient for antioxidant, cytoprotective and antimicrobial activities.

Comparative Analysis of Ginsenoside Content in Processed Red Ginseng Foods Based on Food Type and Formulation (홍삼가공식품의 식품유형별 및 제형별 진세노사이드 함량 비교)

  • Yun-Jeong Yi;Min-Su Chang;In-Sook Lee;Hyun-Jeong Kim;Hyun-Jeong Jang;In-Sook Hwang
    • Journal of Food Hygiene and Safety
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    • v.39 no.2
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    • pp.163-170
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    • 2024
  • Red ginseng is manufactured as a health-functional food and is also present in various food types and in different product forms. However, there is currently no standardized regulation of ginsenoside content in foods containing red ginseng. In the present study, we analyzed the ginsenoside content of 66 red ginseng-containing foods and 35 health-functional foods collected online and directly from the market. The ginsenoside content was assessed using liquid chromatography (LC) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) methods. The ginsenoside content of the various food types ranged 0.0 (not detected)-71.567 mg per daily intake of foods containing red ginseng. Sugar-preserved foods had the highest ginsenoside content, followed by solid teas, liquid teas, and red ginseng beverages. For health-functional foods, the ginsenoside content ranged 3.4-58.5 mg per daily intake, with levels ranging 83-607% of the indicated amounts. All values met the established standards. Upon comparing red ginseng health-functional foods and red ginseng-containing foods, the average ginsenoside content was determined to be 18.21 and 8.79 mg, respectively, thus being nearly twice as high in health-functional foods. However, there was a minimal difference between the ginsenoside content of red and black ginseng, with values of 11.84 and 12.63 mg, respectively. These findings provide insights on the variations in ginsenoside content of red and black ginseng in various food forms. This information is expected to be valuable for future regulations and consumer choice of products containing red ginseng.

Simultaneous Analysis of the Compounds of Natural Cosmetic Resources Containing Chrysanthemum zawadskii, Perilla frutescens, Rosa multiflora and their Anti-oxidative Activity (산구절초, 자소엽, 찔레를 함유한 천연 화장품소재의 다성분 동시분석과 항산화활성)

  • Ham, Ha Neul;Shrestha, Abinash Chandra;Kim, Ju Eun;Lee, Tae Bum;Yoo, Byoung Wan;Kim, Min Sook;Kim, Kwang Sang;Cha, Joon-Seok;Lee, Yong Mun;Kim, Jeong Yeob;Leem, Jae Yoon
    • Korean Journal of Pharmacognosy
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    • v.49 no.4
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    • pp.312-321
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    • 2018
  • Recently, consumer demand for functional cosmetics containing natural ingredients has been greatly expanded. To develop the natural cosmetic materials, we selected 3 plants, Chrysanthemum zawadskii Herbich (CZ), Perilla frutescens (L.) Britton var. acuta Kudo (PF), and Rosa multiflora Thunberg (RM) which showed high total flavonoid contents (TFC), total polyphenol contents (TPC), and strong DPPH radical scavenging effect. We determined astragalin, chlorogenic acid, and rosmarinic acid as a marker compound for quantitative analysis of the content of each material and standardization of the quality standards and manufacturing standards through LC/MS analysis. HPLC-DAD was used to simultaneously analyze these marker components of three natural product complexes (Mix) and to validate the analytical method through experiments such as linearity, accuracy and precision. The detection wavelengths were set at 210, 265, and 330 nm. The detected 3 compounds from extract of CZ, PF, RM showed significant linearity ($R^2${\geq_-}$0.9947). The limit of detection (LOD) of chlorogenic acid, astragalin and rosmarinic acid were $8.29{\mu}g/ml$, $2.28{\mu}g/ml$, and $27.00{\mu}g/ml$, respectively. The limit of quantification (LOQ) of chlorogenic acid, astragalin and rosmarinic acid were $25.11{\mu}g/ml$, $6.92{\mu}g/ml$, and $81.83{\mu}g/ml$, respectively. The contents of the three indicators of Mix were 19.82-24.71 mg/g of chlorogenic acid, 43.80-46.02 mg/g of astragalin, and 46.33-48.57 mg/g of rosmarinic acid.

Translocation of Tolclofos-methyl from Ginseng Cultivated Soil to Ginseng (Panax ginseng C. A. Meyer) and Residue Analysis of Various Pesticides in Ginseng and Soil (토양 중 잔류된 Tolclofos-methyl의 인삼(Panax ginseng C. A. Meyer)에 대한 이행 및 잔류 특성)

  • Kim, Ji Yoon;Kim, Hea Na;Saravanan, Manoharan;Heo, Seong Jin;Jeong, Haet Nim;Kim, Jang Eok;Kim, Kwan Rae;Hur, Jang Hyun
    • The Korean Journal of Pesticide Science
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    • v.18 no.3
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    • pp.130-140
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    • 2014
  • Recently, some of the previous studies reported that tolclofos-methyl is still exist in ginseng cultivated soil, even though it is has been banned for ginseng. Therefore, the current study was aimed to examine the levels of absorption and translocation of tolclofos-methyl from ginseng cultivated soil to ginseng root and leaf stem for the period of 1 year. For this study, ginseng plants were transplanted in pots and treated with $5.0mg\;kg^{-1}$ of tolclofos-methyl (50% WP). At the end of each interval periods (every three months) the samples (soil, roots and leaf stems) were collected and analyzed the absorption and translocation levels of tolclofos-methyl using gas chromatography and mass spectrometry (GC-MS). The limit of quantitation of tolclofos-methyl was found to be $0.02mg\;kg^{-1}$ and 70.0~120.0% recovery was obtained with coefficient of variation of less than 10% regardless of sample types. In this study, a considerable amount of translocation of tolclofos-methyl residues were found in soil (4.28 to $0.06mg\;kg^{-1}$), root (7.09 to $1.54mg\;kg^{-1}$) and leaf stem (0.79 to $0.69mg\;kg^{-1}$). The results show that the tolclofos-methyl was absorbted and translocated from ginseng cultivated soil to ginseng root and ginseng leaf stem and found to be decreased time-coursely. Secondly, we were also analyzed soil, root and leaf stems samples from Hongcheon, Cheorwon, Punggi and Geumsan by GC-MS/MS (172 pesticides), LC-MS/MS (74 pesticides). In this study, 43 different pesticides were detected ($0.01{\sim}7.56mg\;kg^{-1}$) in soil, root and leaf stem. Further, tolclofos-methyl was detected 4 times separately in root sample alone which is less ($0.01{\sim}0.05mg\;kg^{-1}$) than their maximum residual limit (MRL) in ginseng. Consequently, the results from both studies indicate the residues of tolclofos-methyl found in ginseng cultivated soil and ginseng ensuring their safety level. Moreover, long-term evaluations are needed in order to protect the soil as well as ginseng free from tolclofos-methyl residues.

Identification of 5-Hydroxy-3,6,7,8,3',4'-Hexamethoxyflavone from Hizikia fusiforme Involved in the Induction of the Apoptosis Mediators in Human AGS Carcinoma Cells

  • Kim, Min Jeong;Lee, Hye Hyeon;Seo, Min Jeong;Kang, Byoung Won;Park, Jeong Uck;Kim, Kyoung-Sook;Kim, Gi-Young;Joo, Woo Hong;Choi, Yung Hyun;Cho, Young-Su;Jeong, Yong Kee
    • Journal of Microbiology and Biotechnology
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    • v.22 no.12
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    • pp.1665-1672
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    • 2012
  • An 80% ethanol extract of Hizikia fusiforme was obtained and followed by successive fractionation using the organic solvents n-hexane, ethyl acetate, and n-butanol to identify the antioxidative substance. The aqueous part of the nbutanol fractionation step, showing high antioxidative activity, was subjected to reverse-phase liquid chromatography. As a result, a substance purified from a BB-2 fraction showed high antioxidative activity. The m/z 419 [M+H] molecular ion peak in the fraction was observed by the analysis of the ESI-LC/MS spectrum. By the analysis of 1H NMR (500 MHz, DMSO-$d_6$) and $^{13}C$ NMR (125 MHz, DMSO-$d_6$) spectra, a unique compound of the fraction was biochemically identified as a 5-hydroxy-3,6,7,8,3',4'-hexamethoxyflavone (5HHMF). We also investigated the effect of 5HHMF on human gastric AGS carcinoma cells. Western blot analysis suggested that the flavone substantially increased the levels of the death receptor-associated apoptosis mediators Fas, Fas L, FADD, TRADD, and DR4 in a concentration-dependent manner. The levels of Fas, Fas L, TRADD, and DR4 in the cells treated with 5HHMF ($5{\mu}g/ml$) were approximately 26.4-, 12.8-, 6.7-, and 9.8-times higher than those of non-treated cells, respectively. Of note, the level of FADD protein in the cells exposed to 5HHMF ($1{\mu}g/ml$) increased approximately 9.6-times. In addition, the cleavage of caspase-3, -8, and -9 in cultured AGS cells treated with 5HHMF was significantly confirmed. Therefore, our results suggest that 5HHMF from H. fusiforme is involved in the induction of death receptor-associated apoptosis mediators in human gastric AGS carcinoma cells.

Development and Validation of an Analytical Method for Ametoctradin Residue Determination in Domestic Agricultural Commodities by HPLC-PDA (HPLC-PDA를 이용한 국내 유통 농산물 중 ametoctradin 잔류량 분석법 개발 및 검증)

  • Do, Jung-Ah;Kwon, Ji-Eun;Lee, Eun-Mi;Kim, Mi-Ra;Kuk, Ju-Hee;Cho, Yoon-Jae;Kang, Il-Hyun;Kim, Hyung-Su;Kwon, Kisung;Oh, Jae-Ho
    • Korean Journal of Food Science and Technology
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    • v.45 no.3
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    • pp.285-292
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    • 2013
  • This study was carried out to validate the safety of ametoctradin residues in agricultural commodities by developing an official analysis method. An analytical method was developed and validated using HPLC-PDA detectors. The samples were extracted with methanol, subsequently partitioned with dichloromethane and purified with florisil column chromatograph using acetone/hexane (30/70, v/v) as solvent. The method was validated by using grape, hulled rice, mandarin, and potato spiked with ametoctradin at 0.05 and 5.0 mg/kg, and pepper at 0.05 and 2.0 mg/kg. Average recoveries were 76-114.8% with relative standard deviation less than 10%, and the limit of detection and limit of quantification were 0.0125 and 0.05 mg/kg, respectively. The result of recoveries and overall coefficient of variation of the laboratory results from Gwangju regional Food and Drug Administration (FDA) and Daejeon regional FDA was accorded with Codex Alimentarius Commission Guideline (CAC/GL 40). Based on these results, this method was found to be appropriate for ametoctradin residue determination and can be used as the official method of analysis.

Characteristics of Pesticide Residues in Leafy Vegetables Collected from Wholesale and Traditional Markets in Cheongju (청주지역 도매시장과 재래시장 유통 엽채류 중 농약의 잔류 특성)

  • Noh, Hyun-Ho;Lee, Kwang-Hun;Lee, Jae-Yun;Park, Hyo-Kyoung;Park, So-Hyun;Kim, Sun-Ho;Kyung, Kee-Sung
    • The Korean Journal of Pesticide Science
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    • v.15 no.4
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    • pp.453-462
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    • 2011
  • This study was carried out to survey the residual characteristics of pesticides and assess their safety. Nineteen agricultural commodities, collected from wholesale and traditional markets in Cheongju. Nineteen agricultural commodities including perilla leaves were collected from the markets on October 29th, 2010. Total 240 pesticides which can be analyzed by multiresidue analysis method by GLC and HPLC were monitored and the pesticides detected were confirmed by GC-MSD and LC-MS. Five pesticides, alachlor, bifenthrin, endosulfan, procymidone and triflumizole, were detected from five samples, such as welsh onion, leek and celery in case of wholesale market and perilla leaves and welsh onion in case of traditional market. Detection rate of 13.2% was obtained as a result of pesticide analysis but 2.6% of the pesticides detected exceeded their maximum residue limits. The estimated daily intakes (EDIs) and maximum permissible intakes (MPIs) of the pesticides detected were less than 26% and 0.05% of their acceptable daily intakes (ADIs) respectively, representing that residue levels of the pesticides detected would be safe.

Interplay between the Gut Microbiome and Metabolism in Ulcerative Colitis Mice Treated with the Dietary Ingredient Phloretin

  • Ren, Jie;Li, Puze;Yan, Dong;Li, Min;Qi, Jinsong;Wang, Mingyong;Zhong, Genshen;Wu, Minna
    • Journal of Microbiology and Biotechnology
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    • v.31 no.10
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    • pp.1409-1419
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    • 2021
  • A growing number of healthy dietary ingredients in fruits and vegetables have been shown to exhibit diverse biological activities. Phloretin, a dihydrochalcone flavonoid that is abundant in apples and pears, has anti-inflammatory effects on ulcerative colitis (UC) mice. The gut microbiota and metabolism are closely related to each other due to the existence of the food-gut axis in the human colon. To investigate the interplay of faecal metabolites and the microbiota in UC mice after phloretin treatment, phloretin (60 mg/kg) was administered by gavage to ameliorate dextran sulfate sodium (DSS)-induced UC in mice. Gut microbes and faecal metabolite profiles were detected by high-throughput sequencing and liquid chromatography mass spectrometry (LC-MS) analysis, respectively. The correlations between gut microbes and their metabolites were evaluated by Spearman correlation coefficients. The results indicated that phloretin reshaped the disturbed faecal metabolite profile in UC mice and improved the metabolic pathways by balancing the composition of faecal metabolites such as norepinephrine, mesalazine, tyrosine, 5-acetyl-2,4-dimethyloxazole, and 6-acetyl-2,3-dihydro-2-(hydroxymethyl)-4(1H)-pyridinone. Correlation analysis identified the relations between the gut microbes and their metabolites. Proteus was negatively related to many faecal metabolites, such as norepinephrine, L-tyrosine, laccarin, dopamine glucuronide, and 5-acetyl-2,4-dimethyloxazole. The abundance of unidentified Bacteriodales_S24-7_group was positively related to ecgonine, 15-KETE and 6-acetyl-2,3-dihydro-2-(hydroxymethyl)-4(1H)-pyridinone. The abundance of Christensenellaceae_R-7_group was negatively related to the levels of 15-KETE and netilmicin. Stenotrophomonas and 15-KETE were negatively related, while Intestinimonas and alanyl-serine were positively related. In conclusion, phloretin treatment had positive impacts on faecal metabolites in UC mice, and the changes in faecal metabolites were closely related to the gut microbiota.

Development of simultaneous analytical method for investigation of ketamine and dexmedetomidine in feed (사료 내 케타민과 덱스메데토미딘의 잔류조사를 위한 동시분석법 개발)

  • Chae, Hyun-young;Park, Hyejin;Seo, Hyung-Ju;Jang, Su-nyeong;Lee, Seung Hwa;Jeong, Min-Hee;Cho, Hyunjeong;Hong, Seong-Hee;Na, Tae Woong
    • Analytical Science and Technology
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    • v.35 no.3
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    • pp.136-142
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    • 2022
  • According to media reports, the carcasses of euthanized abandoned dogs were processed at high temperature and pressure to make powder, and then used as feed materials (meat and bone meal), raising the possibility of residuals in the feed of the anesthetic ketamine and dexmedetomidine used for euthanasia. Therefore, a simultaneous analysis method using QuEChERS combined with high-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry was developed for rapid residue analysis. The method developed in this study exhibited linearity of 0.999 and higher. Selectivity was evaluated by analyzing blank and spiked samples at the limit of quantification. The MRM chromatograms of blank samples were compared with those of spiked samples with the analyte, and there were no interferences at the respective retention times of ketamine and dexmedetomidine. The detection and quantitation limits of the instrument were 0.6 ㎍/L and 2 ㎍/L, respectively. The limit of quantitation for the method was 10 ㎍/kg. The results of the recovery test on meat and bone meal, meat meal, and pet food showed ketamine in the range of 80.48-98.63 % with less than 5.00 % RSD, and dexmedetomidine in the range of 72.75-93.00 % with less than 4.83 % RSD. As a result of collecting and analyzing six feeds, such as meat and bone meal, prepared at the time the raw material was distributed, 10.8 ㎍/kg of ketamine was detected in one sample of meat and bone meal, while dexmedetomidine was found to have a concentration below the limit of quantitation. It was confirmed that the detected sample was distributed before the safety issue was known, and thereafter, all the meat and bone meal made with the carcasses of euthanized abandoned dogs was recalled and completely discarded. To ensure the safety of the meat and bone meal, 32 samples of the meat and bone meal as well as compound feed were collected, and additional residue investigations were conducted for ketamine and dexmedetomidine. As a result of the analysis, no component was detected. However, through this investigation, it was confirmed that some animal drugs, such as anesthetics, can remain without decomposition even at high temperature and pressure; therefore, there is a need for further investigation of other potentially hazardous substances not controlled in the feed.

NecroX-5 protects mitochondrial oxidative phosphorylation capacity and preserves PGC1α expression levels during hypoxia/reoxygenation injury

  • Vu, Thi Thu;Kim, Hyoung Kyu;Le, Thanh Long;Nyamaa, Bayalagmaa;Song, In-Sung;To, Thanh Thuy;Nguyen, Quang Huy;Marquez, Jubert;Kim, Soon Ha;Kim, Nari;Ko, Kyung Soo;Rhee, Byoung Doo;Han, Jin
    • The Korean Journal of Physiology and Pharmacology
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    • v.20 no.2
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    • pp.201-211
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    • 2016
  • Although the antioxidant and cardioprotective effects of NecroX-5 on various in vitro and in vivo models have been demonstrated, the action of this compound on the mitochondrial oxidative phosphorylation system remains unclear. Here we verify the role of NecroX-5 in protecting mitochondrial oxidative phosphorylation capacity during hypoxia-reoxygenation (HR). Necrox-5 treatment ($10{\mu}M$) and non-treatment were employed on isolated rat hearts during hypoxia/reoxygenation treatment using an ex vivo Langendorff system. Proteomic analysis was performed using liquid chromatography-mass spectrometry (LC-MS) and non-labeling peptide count protein quantification. Real-time PCR, western blot, citrate synthases and mitochondrial complex activity assays were then performed to assess heart function. Treatment with NecroX-5 during hypoxia significantly preserved electron transport chain proteins involved in oxidative phosphorylation and metabolic functions. NecroX-5 also improved mitochondrial complex I, II, and V function. Additionally, markedly higher peroxisome proliferator-activated receptor-gamma coactivator-$1{\alpha}$ ($PGC1{\alpha}$) expression levels were observed in NecroX-5-treated rat hearts. These novel results provide convincing evidence for the role of NecroX-5 in protecting mitochondrial oxidative phosphorylation capacity and in preserving $PGC1{\alpha}$ during cardiac HR injuries.